Hydrochloric Acid → (E)-3-[1-[4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl]-1H-pyrazol-4-yl]propenoic acid

HRID 350150ノート

反応式

HRID 350150 の反応式
[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:33]=[CH:32][C:18]([CH2:19][N:20]2[CH:24]=[C:23](/[CH:25]=[CH:26]/[C:27]([O:29]CC)=[O:28])[CH:22]=[N:21]2)=[CH:17][CH:16]=1.[OH-].[Na+].C(O)C.Cl>O1CCCC1>[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:33]=[CH:32][C:18]([CH2:19][N:20]2[CH:24]=[C:23](/[CH:25]=[CH:26]/[C:27]([OH:29])=[O:28])[CH:22]=[N:21]2)=[CH:17][CH:16]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 69423038ethyl(E)-3-[1-[4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl]-1H-pyrazol-4-yl]propenoate

生成物 1

HCID 69420714(E)-3-[1-[4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl]-1H-pyrazol-4-yl]propenoic acid収率 81%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
40 °C

実験手順

A mixture of ethyl(E)-3-[1-[4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl]-1H-pyrazole-4-yl]propenoate (887 mg), 1 N aqueous sodium hydroxide solution (4 ml), ethanol (8 ml), and tetrahydrofuran (8 ml) was stirred at 40° C. for 3 hours. After the reaction mixture was acidified with 1 N hydrochloric acid, the obtained crystals were collected by filtration, and (E)-3-[1-[4-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl]-1H-pyrazol-4-yl]propenoic acid (672 mg, yield: 81%) was obtained. This was recrystallized from ethanol. Melting point: 186–187° C.

後処理

  1. filtrationthe obtained crystals were collected by filtration

出典と根拠

ORDレコード
ord-88bc325a2a8c464eadcdb25370e2e9c8
出典データセット
uspto-grants-2007_02
特許番号
US07179823B1

反応ノート

読み込み中…